CN104550965B - Method for preparing chromium-based composite material for connecting plate - Google Patents
Method for preparing chromium-based composite material for connecting plate Download PDFInfo
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- CN104550965B CN104550965B CN201310524707.8A CN201310524707A CN104550965B CN 104550965 B CN104550965 B CN 104550965B CN 201310524707 A CN201310524707 A CN 201310524707A CN 104550965 B CN104550965 B CN 104550965B
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Abstract
The invention relates to a method for preparing a chromium-based composite material for a connecting plate. Aluminum oxide is adopted by the chromium-based composite material for replacing Yttrium oxide in a commercial Cr-5Fe-1Y2O3 material, the aluminum oxide in a submicron level can be uniformly and dispersedly arranged in a chromium-based body, chromium oxide crystalline grains are prevented from being thickened and enlarged, and high-temperature oxidation of chromium is slowed down. The method comprises the preparing steps of firstly, preparing aluminum sol coating chromium powder; then mixing the aluminum sol coating chromium powder with alloying elements and a lubricating agent; then, forming in a pressing way; finally, cooling after high-temperature sintering. According to the method for preparing the chromium-based composite material for the connecting plate, disclosed by the invention, the technology is simple, and the prepared chromium-based composite material has excellent high temperature-resisting performance and corrosion resistance; compared with existing commercial Cr-5Fe-1Y2O2, the cost is low, meanwhile, the thermal expansion coefficient is close to that of other components of a solid fuel cell, large influence on assembling and use cannot be generated, the chromium-based composite material can be used as a connecting plate of a fuel cell and is a feasible material for replacing the Cr-5Fe-1Y2O2, and the chromium-based composite material is suitable for being produced in a large scale.
Description
Technical field
The invention belongs to chromium-base alloy technical field of composite materials, it is related to a kind of powder metallurgy aluminium oxide of high temperature application more
Dissipate and strengthen chromio composite, the preparation method of especially a kind of chromio composite being applied to fuel cell connecting board.
Background technology
SOFC is a kind of clean cleaning, efficient, noiseless green energy resource, and energy conversion efficiency is high
Reach 85%, but cell power limited is it is necessary to dress up set of cells by connector by several single battery groups, required to obtain
Power.Connector needs to adopt high temperature oxidation resisting, and electrical and thermal conductivity is good, thermal expansion characteristics and battery other assemblies phase
Join, the material of energy long-term stable operation.Have Cr-5Fe-1Y at present2O3Series material is applied in solid fuel cell field.Oxygen
Role is in the material to change yttrium：Yittrium oxide using disperse stops chromium oxide coarse grains, the oxidation after crystal grain thinning
Chromium is easily formed the chromium oxide layer of densification, slows down further oxidation.It is added to Cr-5Fe-1Y2O3Yittrium oxide in material needs
Micron order or even submicron order magnitude powder, yittrium oxide belongs to rare earth oxide, and price is extremely expensive it is contemplated that connector is work(
Energy structural member, requirement is greatly it is therefore necessary to develop more cheap substitution material.
As conventional exotic material, its fusing point is up to 2000 DEG C to aluminium oxide, and it is cheap.Based on same former
Reason, aluminum oxide dispersion is distributed in chromio body it is contemplated that similar effect also can be played, and stops the coarse grains of chromium oxide, subtracts simultaneously
Slow chromium oxidation.Generally alumina powder particle diameter in 10 μm of magnitudes, with chromium Primary Particle Size（10-100μm）Belong to same amount
Level, if being directly added in chromium-base alloy in the form of alumina powder, is difficult to play the shape stoping big crystal grain size chromium oxide
Become, and be directly added into the shaping density that micron-sized alumina powder can reduce powder metallurgy formation part.Therefore, it is necessary to adopt
Any special measures are taken to make the aluminium oxide around evanohm crystal grain be much smaller than 10 μm.Using sol method cladding, high temperature sintering can be in chromium
Powder coated with uniform alumina particle, cladding thickness is adjustable.In colloidal sol, the size of particle is in 1～1000nm（Wide in range definition,
Also it is defined as 1～100nm）, it is more conform with the requirement that disperse phase size is much smaller than 10 μm.
Content of the invention
The technical problem to be solved is to provide a kind of preparation method of connecting plate chromio composite, has
Process is simple, feature with low cost, prepared material has excellent resistance to elevated temperatures and corrosion resistance.
The present invention solves the technical scheme that adopted of above-mentioned technical problem：A kind of connecting plate system of chromio composite
Preparation Method is it is characterised in that comprise the following steps：
1）Prepare Alumina gel cladding chromium powder；
2）It is mixed after above-mentioned prepared Alumina gel coats and adds alloying element and lubricant according to certain ratio in chromium powder
Close uniformly, alloying element includes but is not limited to one or more of Fe, Ni, Co, W, Mo, Al, Mn, V combination；
3）Above-mentioned mixed-powder is suppressed on shaping press, is molded using common, forming pressure is according to density, gas
Depending on close property, intensity, dimensional tolerance etc. require, forming pressure 400～2000MPa, shaping density 5.3g/cm3～7.0g/cm3；
4）Dewaxing and sintering：It is sintered using continuous sintering furnace or discrete sintering furnace, sintering atmosphere is vacuum
Or pure hydrogen or noble gases, dewaxing temperature can be 300～800 DEG C, and 5～60 minutes time, sintering temperature is 1200～1550 DEG C,
10～200 minutes time；
5）Cooled down after terminating.
As improvement, described step 1）Prepare Alumina gel coat chromium powder detailed process be：
A, alumina sol and deionized water are 0.2～5 according to mass ratio：10 carry out dispersing and dissolving, using 60～90
DEG C heating in water bath simultaneously carries out magnetic agitation, dissolution time 30～120min, and the structural formula of above-mentioned alumina sol is：（Al2O3·
nH2O）.bHX, wherein：Al2O3·nH2O is hydrated alumina, and its coefficient n is 1～3；HX be peptizer, be hydrochloric acid, acetic acid or
One of nitric acid or combinations thereof, its coefficient b is 0.1～0.5.
B, in above-mentioned scattered alumina sol solution add chromium powder, be sufficiently mixed and be slowly heated, until moisture
Basic evaporation, the wherein mass ratio of alumina sol and chromium powder are 1：1000～1：10；
C, the mixed-powder being evaporated is positioned in baking oven carries out redrying, 95～105 DEG C of drying 1.5～2.5h, that is,
Obtain required Alumina gel cladding chromium powder.
Described chromium powder is by one of thermal reduction, carbon thermal reduction, electrolysis or the chromium powder obtained by ball grinding method or many
Plant composition；The particle mean size of described chromium powder is 45～100 μm.
Preferably, the mass ratio that described Alumina gel coats alumina sol in chromium powder is 0.1-5wt%.
Preferably, described step 2）In alloying element be one of Fe, Mo, Mn, W or V or multiple combination, profit
Lubrication prescription is the mixing of one or more of KP-11, stearic acid, zinc stearate or lithium stearate, and the content of alloying element is mixing
The 0.2～6% of material gross mass, lubricant content is the 0.1-0.8% of compound gross mass.
As improvement, described step 3）In compacting be not limited to commonly be molded, also can be become using warm-pressing formation or warm mould
Shape.
Preferably, described step 3）In forming pressure be 600～900Mpa.
Further preferably, described step 3）In forming pressure be 650～800MPa
Preferably, described step 4）In sintering atmosphere be hydrogen or argon, sintering temperature be 1420-1480 DEG C, burn
The knot time is 0.5～2h.
Improve again, described step 5）In cooling using be passed through noble gases force cooling or furnace cooling.
Compared with prior art, it is an advantage of the current invention that：Rare-earth oxidation yttrium is substituted using aluminium oxide, through special technique
Prepare dispersed oxide and strengthen chromio composite, aluminum oxide dispersion is distributed in chromio body, stop the crystal grain of chromium oxide thick
Bigization, slows down chromium high-temperature oxydation.The preparation method process is simple of the present invention, prepared chromio composite has excellent resistance to height
Warm nature energy and corrosion resistance, the more existing business-like Cr-5Fe-1Y of cost2O3Cheap, thermal coefficient of expansion and solid fuel cell simultaneously
Other assemblies are close, will not can use as fuel cell connecting board to assembling with using producing big impact, will be to substitute
Cr-5Fe-1Y2O3Viable material, be suitable for large-scale production.
Brief description
Fig. 1 is the preparation technology figure of the aluminum oxide dispersion enhancing chromio material of the present invention；
Fig. 2 is the SEM photograph of the alumina-coated chromium powder after coating and dry through Alumina gel；
Fig. 3 is the SEM photograph strengthening fracture after chromio material hand breaking through oversintering rear oxidation aluminum disperse；
Fig. 4 is the EDS energy spectrum diagram strengthening chromio material through oversintering rear oxidation aluminum disperse.
Specific embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1：
A kind of connecting plate preparation method of chromio composite, comprises the following steps that：
1）Alumina gel disperses：By alumina sol with 1：3.5 ratio is added in deionized water, and 85 DEG C of water-bath magnetic force stir
Mix dispersion 60min, until Alumina gel is completely dispersed.
2）Chromium powder coats：Chromium powder adds after crossing 100 mesh sieves in scattered Alumina gel, the ratio of chromium powder and alumina sol
For 25：1, strong stirring is simultaneously slowly heated to 80 DEG C, and insulation is until moisture evaporation is complete.
3) cladding powder is dried：Shift above-mentioned Alumina gel cladding powder 100 DEG C of insulation 2h in baking oven to be fully dried.
4) batch mixing：Dried Alumina gel is coated chromium powder end, iron powder, lubricant, according to proportioning in bipyramid or V-arrangement batch mixing
Machine or other batch mixers are mixed.Specific proportioning is as follows：Straight iron powder：5%；Powder lubricant：0.2%；Alumina gel coated composite powder
End 94.8%.
5）Compacting：Above-mentioned mixed-powder is suppressed on shaping press, compacting can be molded using common, shapes pressure
Power is 700MPa, and shaping density is 6.37g/cm3.
6）Dewaxing, sintering and cooling：Dewaxing and sintering integrated vacuum-sintering is carried out, dewaxing temperature is 600 DEG C, the time
20 minutes, sintering temperature was 1450 DEG C, 1 hour time, reversely charging argon during sintering, partial pressure of ar gas 50Kpa, and sintering furnace is as cold as 1200
DEG C, it is passed through argon and force cooling.
7）Analysis and detection：As needed, detection chemical composition and/or metallographic structure and/or other performances.Through Alumina gel
Alumina sol cladding chromium powder pattern after coating and drying is shown in Fig. 2.
The Cr-Al that the present invention is obtained2O3- 5Fe and existing business-like Cr-5Fe-1Y2O3The contrast of mixed powder forming property is shown in
Table 1.The cross-breaking strength that sintering rear oxidation aluminum disperse strengthens chromio material is shown in Table 2.Sintering rear oxidation aluminum disperse strengthens chromio
The fracture apperance of material is shown in Fig. 3.The power spectrum that sintering rear oxidation aluminum disperse strengthens chromio material is shown in Fig. 4.
Table 1 forming property contrasts（Forming pressure：700Mpa）
Table 2 is identical to be shaped and cross-breaking strength contrast under sintering condition
| Composition | Cross-breaking strength (Mpa) |
| Cr-5Fe-1Y2O3 | 184 |
| Cr-Al2O3-5Fe | 161 |
From table 1, table 2, data can draw：Coated by Alumina gel, the shaping density of chromium powder does not decline, after sintering
Aluminum oxide dispersion strengthens mechanical property and the Cr-5Fe-1Y of chromio material2O3Relatively.
Embodiment 2：
A kind of connecting plate preparation method of chromio composite, comprises the following steps that：
1）Alumina gel disperses：By alumina sol with 1：10 ratio is added in deionized water, and 80 DEG C of water-bath magnetic force stir
Mix dispersion 30min, until Alumina gel is completely dispersed.
2）Chromium powder coats：Chromium powder adds after crossing 100 mesh sieves in scattered Alumina gel, the ratio of chromium powder and alumina sol
For 50：1, strong stirring is simultaneously slowly heated to 80 DEG C, and insulation is until moisture evaporation is complete.
3) cladding powder is dried：Shift above-mentioned Alumina gel cladding powder 100 DEG C of insulation 2h in baking oven to be fully dried.
4) batch mixing：Dried Alumina gel is coated chromium powder end, iron powder, tungsten powder, lubricant, according to proportioning in bipyramid or V
Shape batch mixer or other batch mixers are mixed.Specific proportioning is as follows：Straight iron powder：3%；Tungsten powder：2%；Powder lubricant：
0.2%；Alumina gel cladding powder 94.8%.
5）Compacting：Above-mentioned mixed-powder is suppressed on shaping press, compacting can be molded using common, shapes pressure
Power is 700Mpa, and shaping density is 6.36g/cm3.
6）Dewaxing, sintering and cooling：Dewaxing and sintering integrated vacuum-sintering is carried out, dewaxing temperature is 600 DEG C, the time
20 minutes, sintering temperature was 1480 DEG C, 1.5 hours time, reversely charging argon during sintering, partial pressure of ar gas 30Kpa, and sintering furnace is as cold as
1000 DEG C, it is passed through argon and forces cooling.
7）Analysis and detection：As needed, detection chemical composition and/or metallographic structure and/or other performances.
Table 3 forming property contrasts（Forming pressure：700Mpa）
Table 4 is identical to be shaped and cross-breaking strength contrast under sintering condition
| Composition | Cross-breaking strength (Mpa) |
| Cr-5Fe-1Y2O3 | 184 |
| Cr-Al2O3-3Fe-2W | 155 |
From table 3, table 4, data equally can draw the following conclusions：Coated by Alumina gel, the shaping density of chromium powder not under
Fall, sintered rear oxidation aluminum disperse strengthens mechanical property and the Cr-5Fe-1Y of chromio material2O3Relatively.
Embodiment 3：
A kind of connecting plate preparation method of chromio composite, comprises the following steps that：
1）Alumina gel disperses：By alumina sol with 1：10 ratio is added in deionized water, and 80 DEG C of water-bath magnetic force stir
Mix dispersion 30min, until Alumina gel is completely dispersed.
2）Chromium powder coats：Chromium powder adds after crossing 100 mesh sieves in scattered Alumina gel, the ratio of chromium powder and alumina sol
For 100：1, strong stirring is simultaneously slowly heated to 80 DEG C, and insulation is until moisture evaporation is complete.
3) cladding powder is dried：Shift above-mentioned Alumina gel cladding powder 100 DEG C of insulation 2h in baking oven to be fully dried.
4) batch mixing：Add straight iron powder and lubricant in cladding chromium powder after drying, in V-arrangement batch mixer or other batch mixings
Machine is mixed.The addition of straight iron powder and lubricant is preferably 5Wt%, and the addition of lubricant is preferably 0.2Wt%, all with dry
On the basis of cladding chromium powder weight after dry.
5）Compacting：Above-mentioned mixed-powder is suppressed on shaping press, compacting can be molded using common, shapes pressure
Power is 700Mpa, and shaping density is 6.39g/cm3.
6）Dewaxing, sintering and cooling：Dewaxing and sintering integrated vacuum-sintering is carried out, dewaxing temperature is 600 DEG C, the time
20 minutes, sintering temperature was 1480 DEG C, 1.5 hours time, reversely charging argon during sintering, partial pressure of ar gas 30Kpa, and sintering furnace is as cold as
1000 DEG C, it is passed through argon and forces cooling.
7）Analysis and detection：As needed, detection chemical composition, metallographic structure or other performances.
Table 3 forming property contrasts（Forming pressure：700Mpa）
Table 4 is identical to be shaped and cross-breaking strength contrast under sintering condition
| Composition | Cross-breaking strength (Mpa) |
| Cr-5Fe-1Y2O3 | 184 |
| Cr-Al2O3-5Fe | 169 |
From table 3, table 4, data equally can draw the following conclusions：Coated by Alumina gel, the shaping density of chromium powder not under
Fall, sintered rear oxidation aluminum disperse strengthens mechanical property and the Cr-5Fe-1Y of chromio material2O3Relatively.
Claims (8)
1. a kind of preparation method of connecting plate chromio composite is it is characterised in that comprise the following steps：
1) prepare Alumina gel cladding chromium powder；
2) after above-mentioned prepared Alumina gel coats and adds alloying element and lubricant according to certain ratio in chromium powder, mixing is equal
Even, alloying element includes but is not limited to one or more of Fe, Ni, Co, W, Mo, Al, Mn, V combination；
3) above-mentioned mixed-powder is suppressed on shaping press, using common molding, warm-pressing formation or warm contour forming, shaped
Depending on pressure is according to density, air-tightness, intensity, the requirement of dimensional tolerance, forming pressure 400～2000MPa, shaping density
5.3g/cm3～7.0g/cm3；
4) dewax and sinter：It is sintered using continuous sintering furnace or discrete sintering furnace, sintering atmosphere is vacuum or pure
Hydrogen or noble gases, dewaxing temperature is 300～800 DEG C, 5～60 minutes time, and sintering temperature is 1200～1550 DEG C, the time 10
～200 minutes；
5) cooled down after terminating；
Described step 1) detailed process of preparing submicron order alumina-coated chromium powder is：
A, alumina sol and deionized water are 0.2～5 according to mass ratio：10 carry out dispersing and dissolving, using 60～90 DEG C of water
Magnetic agitation, dissolution time 30～120min are heated and carry out in bath, and the structural formula of above-mentioned alumina sol is：(Al2O3·
nH2O) .bHX, Al2O3·nH2O is hydrated alumina, and its coefficient n is 1～3, HX is peptizer, is in hydrochloric acid, acetic acid or nitric acid
One kind or combinations thereof, its coefficient b be 0.1～0.5；
B, in above-mentioned scattered alumina sol solution add chromium powder, be sufficiently mixed and be slowly heated, until moisture is basic
Evaporation, the wherein mass ratio of alumina sol and chromium powder are 1：1000～1：10；
C, the mixed-powder being evaporated is positioned in baking oven carries out redrying, 95～105 DEG C of drying 1.5～2.5h, that is, obtain
Required Alumina gel cladding chromium powder.
2. preparation method according to claim 1 it is characterised in that：Described chromium powder is by thermal reduction, carbon thermal reduction, electrolysis
Or one or more of chromium powder obtained by ball grinding method forms；The particle mean size of described chromium powder is 45～100 μm.
3. preparation method according to claim 1 it is characterised in that：Described Alumina gel coats alumina sol in chromium powder
Mass ratio is 0.1-5wt%.
4. preparation method according to claim 1 it is characterised in that：Described step 2) in alloying element be Fe, Mo,
One of Mn, W or V or multiple combination, lubricant is one of KP-11, stearic acid, zinc stearate or lithium stearate
Or several mixing, the content of alloying element is the 0.2～6% of compound gross mass, and lubricant content is compound gross mass
0.1-0.8%.
5. preparation method according to claim 1 it is characterised in that：Described step 3) in forming pressure be 600～
900Mpa.
6. preparation method according to claim 5 it is characterised in that：Described forming pressure is 650～800MPa.
7. preparation method according to claim 1 it is characterised in that：Described step 4) in sintering atmosphere be hydrogen or argon
Gas, sintering temperature is 1420-1480 DEG C, and sintering time is 0.5～2h.
8. preparation method according to claim 1 it is characterised in that：Described step 5) in cooling using being passed through indifferent gas
Body forces cooling or furnace cooling.
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| CN108941543A (en) * | 2018-09-28 | 2018-12-07 | 长安大学 | A kind of alumina-coated crome metal raw powder's production technology |
| CN111922350B (en) * | 2020-09-22 | 2021-01-01 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of low-hydrochloric-acid-insoluble metal chromium powder |
| CN111922351B (en) * | 2020-09-23 | 2021-01-01 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of high-purity low-oxygen metal chromium powder |
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| CN101226807A (en) * | 2007-09-05 | 2008-07-23 | 湖州科达磁电有限公司 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
| CN101477869A (en) * | 2008-09-23 | 2009-07-08 | 彭亦瑜 | Novel nickel zincium soft magnetic ferrite and manufacturing process thereof |
| CN103334022A (en) * | 2013-06-25 | 2013-10-02 | 西安理工大学 | Preparation method of Al2O3 particle enhanced W/Cr bimetal-based composite material |
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| US20090068055A1 (en) * | 2007-09-07 | 2009-03-12 | Bloom Energy Corporation | Processing of powders of a refractory metal based alloy for high densification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101226807A (en) * | 2007-09-05 | 2008-07-23 | 湖州科达磁电有限公司 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
| CN101477869A (en) * | 2008-09-23 | 2009-07-08 | 彭亦瑜 | Novel nickel zincium soft magnetic ferrite and manufacturing process thereof |
| CN103334022A (en) * | 2013-06-25 | 2013-10-02 | 西安理工大学 | Preparation method of Al2O3 particle enhanced W/Cr bimetal-based composite material |
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